CN107352567A - Method for preparing high-purity aluminum oxide by vacuum reduction, distillation and purification - Google Patents

Method for preparing high-purity aluminum oxide by vacuum reduction, distillation and purification Download PDF

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Publication number
CN107352567A
CN107352567A CN201610299339.5A CN201610299339A CN107352567A CN 107352567 A CN107352567 A CN 107352567A CN 201610299339 A CN201610299339 A CN 201610299339A CN 107352567 A CN107352567 A CN 107352567A
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purity
fine powder
vacuum
reduction
reducing agent
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CN107352567B (en
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陈明彪
王利飞
楚铭
金培鹏
看卓才郎
李振盛
李青山
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Qinghai University
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01FCOMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F7/00Compounds of aluminium
    • C01F7/02Aluminium oxide; Aluminium hydroxide; Aluminates
    • C01F7/46Purification of aluminium oxide, aluminium hydroxide or aluminates
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00Physical properties of inorganic compounds
    • C01P2006/80Compositional purity

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Geology (AREA)
  • Inorganic Chemistry (AREA)
  • Manufacture And Refinement Of Metals (AREA)

Abstract

The method for preparing high-purity aluminum oxide by vacuum reduction distillation purification can be used for purifying industrial grade Al with general purity2O3And (3) fine powder. The characteristic technology is as follows: the method comprises the following steps: (1) with Al of ordinary purity2O3Mixing it with high-purity fine powder of carbonaceous reducing agent in a certain proportion, (2) adding it into vacuum distillation furnace, vacuumizing to a certain vacuum degree, heating to a certain temp. and keeping it, and reduction distilling to make Al2O3Impurity of Na2O、SiO2、Fe2O3、TiO2、ZnO2MgO and CaO are reduced to metals by C in the fine powder of the carbonaceous reducing agent, and Na, Mg and Ca (and crystal H) are formed2O and CO2) Volatilize Al2O3Keeping the Fe solution unreduced, insoluble and volatile, and the Fe solution can be deposited on the A by gravityl2O3Then, (3) collecting the residue after reduction and evaporation, and removing the Fe liquid or solid Fe under the residue to obtain high purity Al2O3Fine powder, and collecting the condensed Na, Zn, Mg and Ca solutions of the evaporated gas by condensation respectively or in a mixed manner.

Description

The method that vacuum reduction distilation prepares high purity aluminium oxide
Technical field
The present invention relates to the process that a kind of vacuum reduction distilation prepares high purity aluminium oxide.
Background technology
High-purity alchlor (Al2O3) it is important raw and processed materials required for the industries such as metallurgy, chemical industry, electronics, typically require its purity to be more than 4N levels;Sapphire crystal needed for LED industry has strict demand to the purity of aluminum oxide, particularly has particular/special requirement to micronutrient levels such as Si, Na, Ca, Mg, Cu, Ti, general to require it is that content is not more than 5ppm.According to《YS7274-1998》The Al of the industrial trade mark of production2O3Raw material (Al2O3- 1, -2, -3, -4, referred to as:Al2O3) purity be generally 2N levels, wherein containing impurity Na2O、SiO2、Fe2O3、TiO2、ZnO2, MgO, CaO etc. (mainly first 4 kinds).It is existing to prepare high-purity Al2O3Method have:Zone melting method, the method equipment is complicated, needs in advance by Al2O3Bar, low production efficiency, cost height is made;Aluminium water direct hydrolysis method, the method technical process control are complicated, it is impossible to are purified, product purity depends on the purity of raw material aluminium fine powder;Alum method, advantage of lower cost, technique are simple, small investment, but produce discharge SO2Gas, pollutes environment, and product purity is low;Aluminium carbonate ammonium method, production cycle length, the bad control of technique, product purity is relatively low, in 4N or so;Aluminium alcoholates salt solution solution, the aluminum oxide purity of production is high, crystal grain is small, but cost height, complex technical process, safety and environmental issue be present;Vacuum cold crucible electromagnetic levitation-melt method, product purity in by raw material oxide impurity content influenceed.Currently without with common Al2O3Product is raw material, and high-purity Al is prepared by vacuum reduction distilation2O3Technology.According to non-ferrous metal vacuum reduction distillation principle, by vacuum reduction distillation certain reducing agent may be used to carry out reduction distillation purification to some metal oxides and prepare high purity metal oxides, product purity is expected to reach more than 4N or 5N levels, and process is simple, equipment is prior art, and cost is low.
Bibliography:
[1] Yongnian, Yang Bin nonferrous materials vacuum metallurgy [M] Beijing are worn:Metallurgical publishing house, 2000.
[2] Liu builds research [D] the Kunming University of Science and Technology thesis for the doctorate that people's pure aluminum Hydrolyze methods prepare high purity aluminium oxide, and 2005:1-40.
[3] Wang Jiao, Li Hongjun, bend skilful chivalrous, Xu Xiaodong, Zhang Daobiao, He Xuemei, and Xu Jun cold crucibles method prepares Al2O3Technological parameter research [J] artificial lens journals of polycrystalline material, 2012,41 (3):578-580.
[4] Lian Jiasong, Li Dongyun, Yang Hui.Green Synthesis of Nanometer γ-Al2O3 Powders by Sol-Gel Method [J] Rare Metals Materials and engineering.2008,37 (supplementary issues 2):334-336.
[5] preparation method [P] .CN201210403743.4 of a kind of α types nano-aluminium oxide particles of Luoyang Normal College,
The content of the invention
The object of the invention:
The present invention provides a kind of method that vacuum reduction distilation prepares high purity aluminium oxide, can be applied to prepare high purity aluminium oxide.
The technical solution of the present invention:
The method that vacuum reduction distilation prepares high purity aluminium oxide, it is characterized in that:It includes step:(1) using the Al of general purity2O3(abbreviation Al2O3), after it is well mixed according to a certain percentage with the carbonaceous reducing agent fine powder of high-purity, (2) are added in vacuum distillation furnace, and electrified regulation to certain temperature and is kept after vacuumizing up to certain vacuum degree, and carrying out reduction distillation makes described Al2O3In impurity Na2O、SiO2、Fe2O3、TiO2、ZnO2, MgO, CaO (mainly first 4 kinds) be reduced to metal by the C in described carbonaceous reducing agent fine powder, and make Na, Mg, Ca (and crystallization H2O and CO2) volatilization, but make Al2O3Holding be not reduced and it is insoluble and volatilization, and Fe liquid can after stopping power supply gravity sedimentation in Al2O3Under, (3) collect the residue after described reduction and described evaporation, and remove the Fe liquid or solid-state Fe under described residue, obtain the high-purity Al of product2O3Powder, and condensing metal Na, Zn, Mg, Ca liquid of boil-off gas that can be respectively or described in condensation by mixing collection are byproduct.
The method that vacuum reduction distilation according to above-mentioned technical solution prepares high purity aluminium oxide, it is characterized in that:Described Al2O3Can be the Al of the industrial trade mark2O3Fine powder body;Described vacuum distillation furnace can carry the evaporator being made up of resistive heating device and crucible, and the single chamber or multiple-chamber type condenser being provided with according to the species of metal gas and its similarities and differences of dew point of volatilization;The carbonaceous reducing agent fine powder of described high-purity can be high purity graphite fine powder or high-purity carbon black fine powder or highly pure active charcoal fine powder;Described certain vacuum and temperature can be 10-1-10-2Pa and 1300-1200 DEG C;Described certain proportion can be according to described Al2O3Na described in fine powder2O、SiO2、Fe2O3、TiO2, ZnO, MgO, CaO accurately determine after accurately being calculated or tested by the required of the reduction completely of the C in described carbonaceous reducing agent fine powder.
The method that vacuum reduction distilation according to above-mentioned technical solution prepares high purity aluminium oxide, it is characterized in that:Described crucible can be corundum crucible.
Usefulness of the present invention:
Vacuum reduction distilation of the present invention prepares the technical method of high purity aluminium oxide, and according to aforementioned techniques solution, described Al can be made by step (1)-(4)2O3Impurity Na in fine powder2O、SiO2、Fe2O3、TiO2、ZnO2, MgO, CaO (mainly first 4 kinds) be reduced to metal by the carbonaceous reducing agent fine powder of high-purity, and make Na, Zn, Mg, Ca evaporative removal therein, but make Al2O3Holding is not reduced and insoluble and volatilization form residue, Fe liquid can gravity sedimentation, after the Fe liquid or solid-state Fe under the residue described in removing, obtain the Al of high-purity2O3Product, can also be in the single chamber or multiple-chamber type condenser described in different respectively or mixing recovery byproduct Na, Zn, Mg, Ca molten metal.Using the carbonaceous reducing agent fine powder of graphite fine powder or activated carbon fine powder or carbon black fines as described high-purity, it is ensured that it is high-purity and easily disperseed and described Al2O3Fine powder is well mixed according to described certain proportion, in favor of complete described reduction reaction occurs;Described certain vacuum and temperature and its be 10-1-10-2Pa and 1300-1200 DEG C, described Al can be both made2O3Described impurity Na in fine powder2O、SiO2、Fe2O3、TiO2、ZnO2, MgO, CaO be reduced, Na, Zn, Mg, Ca (and crystallization H2O and CO2) volatilization, Fe2O3Fe liquid is reduced to, described Al can be made again2O3Al in fine powder2O3Component is not reduced and occurs to volatilize and left behind, and after Fe liquid or solid-state Fe of the gravity sedimentation under described residue is removed, obtains high-purity Al2O3Fine powder product;Described certain proportion, it can both ensure that described reduction reaction occurred completely, by that can prevent in the high-purity Al of product2O3In have the impurity C compositions of residual;Described crucible is that corundum crucible can prevent it from being volatilized in described vacuum distillation or wherein impurity element pollutes the described high-purity Al of product2O3Fine powder;The single chamber or multiple-chamber type condenser being provided with according to the species of the metal gas of volatilization and its similarities and differences of dew point, it can make Na, Zn, Mg, Ca composition in described volatilization gas respectively or condensation by mixing is collected.The product purity prepared using the present invention is expected to reach more than 4N or 5N levels, and process is simple, and equipment is prior art, and cost is low.
Embodiment
Technical solution according to foregoing vacuum reduction distilation of the present invention prepares the technical method of high purity aluminium oxide:Can be previously according to existing vacuum distillation furnace technology, the vacuum distillation furnace (prior art) described in selection, the single chamber or multiple-chamber type condenser that prepare the species of metal gas and its similarities and differences of dew point with the evaporator being made up of resistive heating device and corundum crucible and according to volatilization and be provided with;Calculate described impurity Na2O、SiO2、Fe2O3、ZnO2、TiO2, MgO, CaO be reduced sufficiently required described certain proportion.Then:(1) using the Al of the industrial trade mark2O3Fine powder body (abbreviation Al2O3), after it is well mixed with the carbonaceous reducing agent fine powder high purity graphite fine powder or high-purity carbon black fine powder or highly pure active charcoal fine powder of described high-purity according to described certain proportion, (2) add in vacuum distillation furnace, it is 10 to vacuumize up to described certain vacuum-1-10-2Electrified regulation to described certain temperature is 1300-1200 DEG C and kept that carrying out reduction distillation makes described Al after Pa2O3In impurity Na2O、SiO2、Fe2O3、ZnO2、TiO2, MgO, CaO metal is reduced to by the C in described carbonaceous reducing agent fine powder, and make Na, Zn, Mg, Ca (and crystallization H2O and CO2) volatilization, but make Al2O3Holding is not reduced and volatilizees and be in solid fine powder, and Fe be in a liquid state (can gravity sedimentation in Al2O3Under fine powder), (3) collect the residue after described reduction and described evaporation, after the Fe liquid or solid-state Fe under described residue is removed, you can obtain the high-purity Al of product2O3Fine powder, and can be in described single chamber or multiple-chamber type condenser, condensing metal Na, Zn, Mg, Ca liquid of the boil-off gas respectively or described in condensation by mixing collection are byproduct.
The application method of the present invention:
The above-mentioned technical solution and embodiment of the method for high purity aluminium oxide are prepared according to vacuum reduction distilation of the present invention, can be previously according to existing vacuum distillation furnace technology, the vacuum distillation furnace described in selection, the single chamber or multiple-chamber type condenser that prepare the species of metal gas and its similarities and differences of dew point with the evaporator being made up of resistive heating device and corundum crucible and according to volatilization and be provided with;Calculate described impurity Na2O、SiO2、Fe2O3、ZnO2、TiO2, MgO, CaO be reduced sufficiently required described certain proportion;;Then, to the Al of the industrial trade mark2O3Described step (1) -- (3) are carried out, so as to prepare high-purity Al2O3Fine powder, and it is byproduct to collect metal Na, Zn, Mg, Ca liquid.
Embodiment one:The technical solution and embodiment of the invention described above of the technical method of high purity aluminium oxide are prepared according to vacuum reduction distilation of the present invention, can be previously according to existing vacuum distillation furnace technology, the vacuum distillation furnace described in selection, the single chamber or multiple-chamber type condenser that prepare the species of metal gas and its similarities and differences of dew point with the evaporator being made up of resistive heating device and corundum crucible and according to volatilization and be provided with;Calculate described impurity Na2O、SiO2、Fe2O3、ZnO2、TiO2, MgO, CaO be reduced sufficiently required described certain proportion.Then:(1) using the Al of the industrial trade mark2O3Fine powder body (abbreviation Al2O3), after it is well mixed with the carbonaceous reducing agent fine powder high purity graphite fine powder or high-purity carbon black fine powder or highly pure active charcoal fine powder of described high-purity according to described certain proportion, (2) add in vacuum distillation furnace, it is 10 to vacuumize up to described certain vacuum-1Electrified regulation to described certain temperature is 1300 DEG C and kept that carrying out reduction distillation makes described Al after Pa2O3In impurity Na2O、SiO2、Fe2O3、ZnO2、TiO2, MgO, CaO metal is reduced to by the C in described carbonaceous reducing agent fine powder, and make Na, Zn, Mg, Ca (and crystallization H2O and CO2) volatilization, but make Al2O3Holding is not reduced and volatilizees and be in solid fine powder, and Fe be in a liquid state (can gravity sedimentation in Al2O3Under fine powder), (3) collect the residue after described reduction and described evaporation, after the Fe liquid or solid-state Fe under described residue is removed, you can obtain the high-purity Al of product2O3Fine powder, and can be in described single chamber or multiple-chamber type condenser, condensing metal Na, Zn, Mg, Ca liquid of the boil-off gas respectively or described in condensation by mixing collection are byproduct.
Embodiment two:Vacuum reduction distilation according to the technical solution and embodiment of the invention described above prepares the technical method of high purity aluminium oxide, wherein one of described determine vacuum and described certain temperature for 10-2Pa and 1200 DEG C, remaining is identical with embodiment one.

Claims (3)

1. the method that vacuum reduction distilation prepares high purity aluminium oxide, it is characterized in that:It includes step:(1) using the Al of general purity2O3, After it is well mixed according to a certain percentage with the carbonaceous reducing agent fine powder of high-purity, (2) are added in vacuum distillation furnace, are vacuumized up to certain vacuum degree Electrified regulation to certain temperature and is kept afterwards, and carrying out reduction distillation makes described Al2O3In impurity Na2O、SiO2、Fe2O3、TiO2、ZnO2、 MgO, CaO are reduced to metal by the C in described carbonaceous reducing agent fine powder, and make Na, Mg, Ca (and crystallization H2O) volatilize, but make Al2O3Holding be not reduced and it is insoluble and volatilization, and Fe liquid can after stopping power supply gravity sedimentation in Al2O3Under, described in (3) collection also Residue after former and described evaporation, and Fe liquid or solid-state Fe under described residue are removed, obtain the high-purity Al of product2O3Powder, and can divide Condensing metal Na, Zn, Mg, Ca liquid of boil-off gas not or described in condensation by mixing collection are byproduct.
2. the method that vacuum reduction distilation according to claim 1 prepares high purity aluminium oxide, it is characterized in that:Described certain purity Al2O3For the Al of the industrial trade mark2O3Fine powder body;Described vacuum distillation furnace carries the evaporator that is made up of resistive heating device and crucible, and according to The species of the metal gas of volatilization and its similarities and differences of dew point and the single chamber or multiple-chamber type condenser being provided with;The carbonaceous reducing agent of described high-purity is thin Powder is high purity graphite fine powder or high-purity carbon black fine powder or highly pure active charcoal fine powder;Described certain vacuum and temperature is 10-1-10-2Pa and 1300-1200℃;Described certain proportion is according to described Al2O3Na described in fine powder2O、SiO2、Fe2O3、TiO2、ZnO、MgO、 CaO is accurately determined after accurately calculating or test needed for the reduction completely of the C in described carbonaceous reducing agent fine powder.
3. the method that vacuum reduction distilation according to claim 2 prepares high purity aluminium oxide, it is characterized in that:Described crucible is corundum Crucible.
CN201610299339.5A 2016-05-09 2016-05-09 Method for preparing high-purity aluminum oxide by vacuum reduction, distillation and purification Expired - Fee Related CN107352567B (en)

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Cited By (1)

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JPWO2020137875A1 (en) * 2018-12-28 2021-11-25 Dic株式会社 Plate-shaped alumina particles, method for producing plate-shaped alumina particles, and resin composition.

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Publication number Priority date Publication date Assignee Title
JPWO2020137875A1 (en) * 2018-12-28 2021-11-25 Dic株式会社 Plate-shaped alumina particles, method for producing plate-shaped alumina particles, and resin composition.
JP7459801B2 (en) 2018-12-28 2024-04-02 Dic株式会社 Plate-like alumina particles, method for producing plate-like alumina particles, and resin composition

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